CN105609313B - A kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer - Google Patents
A kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer Download PDFInfo
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- CN105609313B CN105609313B CN201610023533.0A CN201610023533A CN105609313B CN 105609313 B CN105609313 B CN 105609313B CN 201610023533 A CN201610023533 A CN 201610023533A CN 105609313 B CN105609313 B CN 105609313B
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- CN
- China
- Prior art keywords
- treatment fluid
- manufacture method
- guide layer
- tantalum capacitor
- coupling agent
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 58
- 239000003990 capacitor Substances 0.000 title claims abstract description 40
- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 36
- 239000002322 conducting polymer Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000012530 fluid Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910002012 Aerosil® Inorganic materials 0.000 claims abstract description 35
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 35
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920000642 polymer Polymers 0.000 claims abstract description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 28
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 18
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical class COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910000077 silane Inorganic materials 0.000 claims description 18
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 14
- 229920001296 polysiloxane Polymers 0.000 claims description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
- 239000004593 Epoxy Substances 0.000 claims description 12
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 12
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 11
- 150000004678 hydrides Chemical class 0.000 claims description 10
- 150000002576 ketones Chemical class 0.000 claims description 9
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 150000001298 alcohols Chemical class 0.000 claims description 7
- 150000002170 ethers Chemical class 0.000 claims description 7
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 6
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 6
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 6
- XOBKSJJDNFUZPF-UHFFFAOYSA-N Methoxyethane Chemical compound CCOC XOBKSJJDNFUZPF-UHFFFAOYSA-N 0.000 claims description 6
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 6
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 6
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 6
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 claims description 6
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 6
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Chemical group CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 5
- 125000002252 acyl group Chemical group 0.000 claims description 5
- 125000004104 aryloxy group Chemical group 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 5
- BBXVGZSHLMEVIP-UHFFFAOYSA-N dodecylsilane Chemical compound CCCCCCCCCCCC[SiH3] BBXVGZSHLMEVIP-UHFFFAOYSA-N 0.000 claims description 5
- 125000003700 epoxy group Chemical group 0.000 claims description 5
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 claims description 5
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 5
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- WALGNFUUHPPUJM-UHFFFAOYSA-N [Si]CCCOC(=O)C=C Chemical compound [Si]CCCOC(=O)C=C WALGNFUUHPPUJM-UHFFFAOYSA-N 0.000 claims description 3
- 125000003545 alkoxy group Chemical group 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 67
- 239000010408 film Substances 0.000 description 34
- -1 carbon alkane Epoxide Chemical group 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 14
- 239000007822 coupling agent Substances 0.000 description 14
- 230000007062 hydrolysis Effects 0.000 description 9
- 238000006460 hydrolysis reaction Methods 0.000 description 9
- 229960000583 acetic acid Drugs 0.000 description 7
- 239000012362 glacial acetic acid Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- MCEBKLYUUDGVMD-UHFFFAOYSA-N [SiH3]S(=O)=O Chemical compound [SiH3]S(=O)=O MCEBKLYUUDGVMD-UHFFFAOYSA-N 0.000 description 2
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000013047 polymeric layer Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000012675 alcoholic extract Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/0425—Electrodes or formation of dielectric layers thereon characterised by the material specially adapted for cathode
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, comprise the following steps：By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, taken out after impregnating 1~20min with the speed of 0.01~5.0mm/min, 5~30min is placed at a temperature of 20~30 DEG C, and drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at 50~260 DEG C；Wherein described treatment fluid includes the solvent of the silane coupling agent that percentage by weight is 0.005~2.0%, 0.01~0.1% aerosil, 3~15% water and surplus.The chip conducting polymer tantalum capacitor cathode guide layer manufactured by the manufacturing method of the present invention has high power capacity extraction rate, low-loss, low ESR and the small characteristic of leakage current come the chip polymer tantalum capacitor that further prepares.
Description
Technical field
The present invention relates to a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer.
Background technology
Due to Ta2O5Dielectric oxide film has oil repellency, and deielectric-coating micropore size skewness, for not preparing guiding
Large aperture (＞ 300nm) medium micropore of layer, this kind of micropore surface implantation adsorbent solution weight is less or flows due to gravity
Other positions are suspended to, therefore the conductive polymer coating for polymerizeing formation is not discontinuous, fine and close, reduces the electric conductivity of polymeric layer
Energy.The tantalum anode block of cathode layer carrier manufacture is not carried out, has even been coated to polymeric layer, interlayer easily occurs after heat-shock
Interfacial separation causes interlayer contact resistance to increase and the equivalent series resistance (ESR) of product is become larger.
The content of the invention
In order to solve the above technical problems, the present invention proposes a kind of system of chip conducting polymer tantalum capacitor cathode guide layer
Method is made, is further prepared by the chip conducting polymer tantalum capacitor cathode guide layer of the manufacturing method of the present invention manufacture
Chip polymer tantalum capacitor there is high power capacity extraction rate, low-loss, low ESR and the small characteristic of leakage current.
To reach above-mentioned purpose, the present invention uses following technical scheme：
The invention discloses a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, including following step
Suddenly：By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, with 0.01~5.0mm/ after 1~20min of dipping
The speed of min is taken out, and 5~30min is placed at a temperature of 20~30 DEG C, and drying and forming-film forms chip at 50~260 DEG C
Conducting polymer tantalum capacitor cathode guide layer；Wherein described treatment fluid includes the silane that percentage by weight is 0.005~2.0%
Coupling agent, 0.01~0.1% aerosil, the solvent of 3~15% water and surplus.
Preferably, the solvent includes at least one of alcohols, ketone, ethers.
Preferably, the solvent includes methanol, ethanol, propyl alcohol, isopropanol, n-butanol, isobutanol, amylalcohol, lauryl alcohol, third
In ketone, butanone, isophorone, methyl ether, ether, butyl ether, ethylene glycol monobutyl ether, methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole at least
It is a kind of.
Preferably, the general formula of the silane coupling agent is RnSiX4-n, wherein R is octenyl, dodecyl, urea groups, carbon alkane
Epoxide, cation alkyl, vinyl, amino, epoxy group, sulfydryl or acryloxypropyl, X for alkoxy, aryloxy group, acyl group,
Methoxy or ethoxy.
Preferably, the silane coupling agent is amino silane, hydrosulphonyl silane, epoxy radicals silicone hydride, vinyl silanes, acryloyl
At least one of oxygen propyl group silane, dodecyl silane.
Preferably, the treatment fluid includes the silane coupling agent, 0.01~0.05% that percentage by weight is 0.1~1.5%
Aerosil, the solvent of 4~10% water and surplus.
Preferably, the treatment fluid includes the silane coupling agent, 0.01~0.05% that percentage by weight is 0.3~1.0%
Aerosil, the solvent of 5~8% water and surplus.
Preferably, by surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid after taking-up, at 20~25 DEG C
At a temperature of place 20min, and drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide at 170~210 DEG C
Layer.
The invention also discloses a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, including it is following
Step：By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, impregnate after 1~20min with 0.01~
The speed of 5.0mm/min is taken out, the temperature at 20~30 DEG C, 60~360min of placement under the humidity of 50%RH~100%RH, and
Drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at 50~260 DEG C；Wherein described treatment fluid includes
The solvent of silane coupling agent, 0.01~0.1% aerosil and surplus that percentage by weight is 0.005~2.0%.
Preferably, the solvent includes at least one of alcohols, ketone, ethers.
Preferably, the solvent includes methanol, ethanol, propyl alcohol, isopropanol, n-butanol, isobutanol, amylalcohol, lauryl alcohol, third
In ketone, butanone, isophorone, methyl ether, ether, butyl ether, ethylene glycol monobutyl ether, methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole at least
It is a kind of.
Preferably, the general formula of the silane coupling agent is RnSiX4-n, wherein R is octenyl, dodecyl, urea groups, carbon alkane
Epoxide, cation alkyl, vinyl, amino, epoxy group, sulfydryl or acryloxypropyl, X for alkoxy, aryloxy group, acyl group,
Methoxy or ethoxy.
Preferably, the silane coupling agent is amino silane, hydrosulphonyl silane, epoxy radicals silicone hydride, vinyl silanes, acryloyl
At least one of oxygen propyl group silane, dodecyl silane.
Preferably, the treatment fluid includes the silane coupling agent, 0.01~0.05% that percentage by weight is 0.1~1.5%
Aerosil and surplus solvent.
Preferably, the treatment fluid includes the silane coupling agent, 0.01~0.05% that percentage by weight is 0.3~1.0%
Aerosil and surplus solvent.
Preferably, by surface attachment Ta2O5The anode tantalum block of dielectric layer be impregnated in treatment fluid take out after, 20~25 DEG C,
120~180min is placed at a temperature of the humidity of 60%RH~90%RH, and drying and forming-film forms chip at 170~210 DEG C
Conducting polymer tantalum capacitor cathode guide layer.
Compared with prior art, the beneficial effects of the present invention are：By the way that Ta will be adhered in a kind of scheme of the present invention2O5
The anode tantalum block of dielectric layer is impregnated in the neutral processing including silane coupling agent, aerosil, solvent and low water content
In liquid, wherein solvent has capillary siphoning effect in the micro channel of dielectric layer so that silane is abundant in dielectric layer surface
Infiltration, absorption；And silane coupling agent, in the neutral liquid of low water content, its hydrolysis rate is eased so that silane coupled
Agent can be hydrolyzed again after by dielectric layer surface fully penetrated, absorption, the silicone hydroxyl formed after hydrolysis, and silane coupled
The organo-functional group included in agent promotes guide layer and conductive polymer layer to have stronger affinity；Also pass through reaction temperature at the same time
The hydrolysis rate of silane coupling agent, and dehydration synthesis guide layer at high temperature are controlled, promotes the interface of guide layer and dielectric layer to melt
Close, so as to improve continuity, the compactness that conducting polymer film layer is coated to.By that will adhere in another scheme of the present invention
Ta2O5The anode tantalum block of dielectric layer be impregnated in including silane coupling agent, aerosil, solvent neutral treatment fluid in, wherein
Solvent has capillary siphoning effect in the micro channel of dielectric layer so that silane is in dielectric layer surface fully penetrated, absorption；
And silane coupling agent is hydrolyzed under higher ambient humidity with the moisture in air, its hydrolysis rate is eased so that silicon
Alkane coupling agent can be hydrolyzed again after by dielectric layer surface fully penetrated, absorption, the silicone hydroxyl formed after hydrolysis, and silicon
The organo-functional group included in alkane coupling agent promotes guide layer and conductive polymer layer to have stronger affinity；At the same time also by anti-
Answer the hydrolysis rate of temperature control silane coupling agent, and dehydration synthesis guide layer at high temperature, promote guide layer and dielectric layer
Interface fusion, so as to improve continuity, compactness that conducting polymer film layer is coated to.It is in addition, few by being added in treatment fluid
The aerosil of amount, can cause aerosil to form good inorganic interface fusion with silane coupling agent,
The Electrical Indexes of invalid micropore influence capacitor can be prevented with micropore invalid in filled media layer；Pass through the present invention's
The chip conducting polymer tantalum capacitor cathode guide layer of manufacture method manufacture is come the chip polymer tantalum capacitance that further prepares
Utensil has high power capacity extraction rate, low-loss, low ESR and the small characteristic of leakage current.
In further scheme, it is R that silane coupling agent, which selects general formula,nSiX4-nMaterial, wherein R select and polymer
Molecule has the group of stronger affinity or respond, and X selects hydrolyzable groups, further improves guide layer and gather with conduction
The affinity of layer is closed, further improves continuity, the compactness that conducting polymer film layer is coated to.
Embodiment
Below and the invention will be further described with reference to preferred embodiment.
The present invention provides a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, in a kind of embodiment party
In formula, including：By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, impregnate after 1~20min with 0.01~
The speed of 5.0mm/min is taken out, and 5~30min, and the drying and forming-film shape at 50~260 DEG C are placed at a temperature of 20~30 DEG C
Into chip conducting polymer tantalum capacitor cathode guide layer；It is 0.005~2.0% that wherein described treatment fluid, which includes percentage by weight,
Silane coupling agent, 0.01~0.1% aerosil, the solvent of 3~15% water and surplus.
Wherein solvent can be at least one of alcohols, ketone, ethers, and alcohols includes methanol, ethanol, propyl alcohol, isopropyl
Alcohol, n-butanol, isobutanol, amylalcohol, lauryl alcohol etc.；Ketone includes acetone, butanone, isophorone etc., and ethers includes methyl ether, second
Ether, butyl ether, ethylene glycol monobutyl ether, methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole etc..
In some preferred embodiments, the general formula of the silane coupling agent is RnSiX4-n, wherein R for it is non-hydrolytic,
The organo-functional group that can be combined with high molecular polymer, according to the heterogeneity of high molecular polymer, R of the invention is preferably used
There are stronger affinity or respond with polymer molecule, can be octenyl, dodecyl, urea groups, carbon alkoxy, sun
Ion alkyl, vinyl, amino, epoxy group, sulfydryl or acryloxypropyl etc.；X uses hydrolyzable groups, can be alcoxyl
Base, aryloxy group, acyl group, methoxy or ethoxy etc..In other embodiments, silane coupling agent is amino silane, sulfydryl silicon
At least one of alkane, epoxy radicals silicone hydride, vinyl silanes, acryloxypropyl silane, dodecyl silane.
In other preferred embodiments, treatment fluid can be comprising the silane that percentage by weight is 0.1~1.5%
Coupling agent, 0.01~0.05% aerosil, the solvent of 4~10% water and surplus, it is highly preferred that treatment fluid includes
The silane coupling agent, 0.01~0.05% aerosil, 5~8% water and remaining that percentage by weight is 0.3~1.0%
The solvent of amount.
In some other embodiment, the manufacturing method of the present invention is included surface attachment Ta2O5The anode tantalum of dielectric layer
Block is impregnated in treatment fluid after taking-up, and 20min, and the drying and forming-film shape at 170~210 DEG C are placed at a temperature of 20~25 DEG C
Into chip conducting polymer tantalum capacitor cathode guide layer；Further, 20min is placed at a temperature of 25 DEG C, and 170~
Drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at 200 DEG C.
The manufacture method of chip conducting polymer tantalum capacitor cathode guide layer provided by the invention, in another embodiment party
In formula, including：By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, impregnate after 1~20min with 0.01~
The speed of 5.0mm/min is taken out, the temperature at 20~30 DEG C, 60~360min of placement under the humidity of 50%RH~100%RH, and
Drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at 50~260 DEG C；Wherein described treatment fluid includes
The solvent of silane coupling agent, 0.01~0.1% aerosil and surplus that percentage by weight is 0.005~2.0%.
Wherein solvent can be at least one of alcohols, ketone, ethers, and alcohols includes methanol, ethanol, propyl alcohol, isopropyl
Alcohol, n-butanol, isobutanol, amylalcohol, lauryl alcohol etc.；Ketone includes acetone, butanone, isophorone etc., and ethers includes methyl ether, second
Ether, butyl ether, ethylene glycol monobutyl ether, methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole etc..
In some preferred embodiments, the general formula of the silane coupling agent is RnSiX4-n, wherein R for it is non-hydrolytic,
The organo-functional group that can be combined with high molecular polymer, according to the heterogeneity of high molecular polymer, R of the invention is preferably used
There are stronger affinity or respond with polymer molecule, can be octenyl, dodecyl, urea groups, carbon alkoxy, sun
Ion alkyl, vinyl, amino, epoxy group, sulfydryl or acryloxypropyl etc.；X uses hydrolyzable groups, can be alcoxyl
Base, aryloxy group, acyl group, methoxy or ethoxy etc..In other embodiments, silane coupling agent is amino silane, sulfydryl silicon
At least one of alkane, epoxy radicals silicone hydride, vinyl silanes, acryloxypropyl silane, dodecyl silane.
In other preferred embodiments, treatment fluid can be comprising the silane that percentage by weight is 0.1~1.5%
The solvent of coupling agent, 0.01~0.05% aerosil and surplus, it is highly preferred that treatment fluid is comprising percentage by weight
The solvent of 0.3~1.0% silane coupling agent, 0.01~0.05% aerosil and surplus.
In some other embodiment, the manufacturing method of the present invention is included surface attachment Ta2O5The anode tantalum of dielectric layer
Block is impregnated in taken out in treatment fluid after, temperature at 20~25 DEG C, place 120 under the humidity of 60%RH~90%RH~
180min, and drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at 170~210 DEG C；Further,
Temperature at 25 DEG C, place 120min under the humidity of 85%RH, and to form chip conductive poly- for drying and forming-film at 170~200 DEG C
Compound tantalum capacitor cathode guide layer.
It is below that the invention will be further described for specific embodiment to manufacture tantalum capacitor of the specification as 16V100 μ F.
Embodiment one：
1) tantalum powder that specific volume is 50000 μ FV/g is conventionally pressed into tantalum briquet, then burnt according to a conventional method
Form anode tantalum block；
2) anode tantalum block is impregnated in salpeter solution according to a conventional method and prepares Ta2O5Dielectric layer；
3) Ta will be prepared2O5The anode tantalum block of dielectric layer is impregnated in low water content, solvent, silica modified processing
In liquid, taken out after impregnating 15min by the speed of 1.0mm/min；Wherein pretreatment fluid is prepared by the raw material of following percetage by weight
Form：Amino silicane coupling agent 1.0%, aerosil 0.01%, water 5%, methanol 60%, n-butanol 33.99%；25
20min, and the drying and forming-film at 180 DEG C are placed at DEG C；
4) conducting polymer thin film is synthesized as cathode guide on the anode tantalum block surface by pretreatment according to a conventional method
Layer；
5) layer surface impregnated graphite and silver paste are guided in polymer cathode according to a conventional method, drying and forming-film, then uses lead
Frame is assembled into tantalum capacitor.
Embodiment two：
Difference lies in the dip time in step 3) is 10min, and treatment fluid includes with embodiment one：Epoxy radicals silicone hydride
Coupling agent 0.3%, aerosil 0.01%, water 5%, ethanol 60%, isopropanol 34.69%.Placed at 25 DEG C
20min, and the drying and forming-film at 170 DEG C.
Embodiment three：
Difference lies in the dip time in step 3) is 10min, and treatment fluid includes with embodiment one：Amino silane is even
Join agent 0.6%, epoxy radicals silicone hydride 0.2%, aerosil 0.02%, water 6%, methanol 56%, propyl alcohol 37.18%.25
20min, and the drying and forming-film at 190 DEG C are placed at DEG C.
Example IV：
Difference lies in the dip time in step 3) is 8min, and treatment fluid includes with embodiment one：Hydrosulphonyl silane is coupled
Agent 0.8%, aerosil 0.01%, water 6%, ethanol 56%, acetone 8.19%, isobutanol 29%.Placed at 25 DEG C
20min, and the drying and forming-film at 200 DEG C.
Embodiment five：
Difference lies in the dip time in step 3) is 8min, and treatment fluid includes with embodiment one：Epoxy radicals silicone hydride is even
Join agent 0.8%, aerosil 0.03%, water 7%, ethanol 50%, isopropanol 42.17%.20min is placed at 25 DEG C,
And the drying and forming-film at 190 DEG C.
Embodiment six：
Difference lies in the dip time in step 3) is 10min, and treatment fluid includes with embodiment one：Vinyl silanes
Coupling agent 0.7%, aerosil 0.02%, water 5%, methanol 58%, ether 6.28%, isopropanol 30%.At 25 DEG C
Place 20min, and the drying and forming-film at 180 DEG C.
Embodiment seven：
Difference lies in the dip time in step 3) is 15min, and treatment fluid includes with embodiment one：Amino silane is even
Join agent 1.0%, aerosil 0.01%, methanol 65%, n-butanol 33.99%.At 25 DEG C of temperature and 80%RH humidity
Place 120min, and the drying and forming-film at 180 DEG C.
Embodiment eight：
Difference lies in the dip time in step 3) is 20min, and treatment fluid includes with embodiment one：Amino silane is even
Join agent 0.3%, aerosil 0.01%, methanol 65%, n-butanol 34.69%；At 20 DEG C of temperature and 90%RH humidity
Place 180min, and the drying and forming-film at 170 DEG C.
Embodiment nine：
Difference lies in the dip time in step 3) is 30min, and treatment fluid includes with embodiment one：Epoxy radicals silicone hydride
Coupling agent 0.1%, amino silicane coupling agent 0.3%, aerosil 0.01%, ethanol 63%, isopropanol 36.59%.
180min, and the drying and forming-film at 170 DEG C are placed at 25 DEG C of temperature and 85%RH humidity.
Embodiment ten：
Difference lies in the dip time in step 3) is 20min, and treatment fluid includes with embodiment one：Vinyl silanes
Coupling agent 0.16%, amino silicane coupling agent 0.3%, aerosil 0.01%, ethanol 63%, isopropanol 36.53%.
180min, and the drying and forming-film at 150 DEG C are placed at 25 DEG C of temperature and 80%RH humidity.
Embodiment 11：
Difference lies in the dip time in step 3) is 25min, and treatment fluid includes with embodiment one：Vinyl silanes
Coupling agent 0.13%, epoxy silane coupling 0.45%, aerosil 0.01%, ethanol 62%, isopropanol
37.41%.120min, and the drying and forming-film at 180 DEG C are placed at 30 DEG C of temperature and 85%RH humidity.
Embodiment 12：
Difference lies in the dip time in step 3) is 25min, and treatment fluid includes with embodiment one：Hydrosulphonyl silane is even
Join agent 0.8%, aerosil 0.01%, ethanol 59%, n-butanol 40.19%.At 25 DEG C of temperature and 90%RH humidity
Place 180min, and the drying and forming-film at 200 DEG C.
Comparative example one：
Difference lies in the dip time in step 3) is 15min, and treatment fluid includes with embodiment one：Amino silane is even
Join agent 1.5%, glacial acetic acid 0.02%, water 90%, methanol 8.48%.20min is placed at 25 DEG C, and is dried at 200 DEG C
Film.
Comparative example two：
Difference lies in the dip time in step 3) is 10min, and treatment fluid includes with embodiment one：Epoxy radicals silicone hydride
Coupling agent 1.8%, glacial acetic acid 0.03%, water 87%, ethanol 11.17%.20min is placed at 25 DEG C, and it is dry at 170 DEG C
Film forming.
Comparative example three：
Difference lies in the dip time in step 3) is 15min, and treatment fluid includes with embodiment one：Amino silane is even
Join agent 1.8wt%, glacial acetic acid 0.03wt%, water 98.17wt%.20min, and the drying and forming-film at 190 DEG C are placed at 25 DEG C.
Comparative example four：
Difference lies in the dip time in step 3) is 15min, and treatment fluid includes with embodiment one：Hydrosulphonyl silane is even
Join agent 2.0%, glacial acetic acid 0.05%, water 97.95%.20min, and the drying and forming-film at 200 DEG C are placed at 25 DEG C.
Comparative example five：
Difference lies in, the dip time in step 3) it is 10min with embodiment one, the amino silane coupling in treatment fluid
Agent 1.0%, epoxy silane coupling 0.8%, glacial acetic acid 0.05%, water 90%, propyl alcohol 8.15%.Placed at 25 DEG C
20min, and the drying and forming-film at 190 DEG C.
Comparative example six：
Difference lies in, the dip time in step 3) it is 20min with embodiment one, the vinyl silanes in treatment fluid are even
Join agent 2.0%, glacial acetic acid 0.15%, water 97.85%.20min, and the drying and forming-film at 170 DEG C are placed at 25 DEG C.
The correction data such as table 1 below of electrical testing is carried out to the tantalum capacitor of above-described embodiment and comparative example manufacture.
1 embodiment of table and the 16V100 μ F tantalum capacitor parameter lookup tables of comparative example manufacture
| Project | Capacity extraction rate (%) | It is lost (%) | ESR(mΩ) | Leakage current (μ A) |
| Embodiment one | 91.2 | 1.9 | 28 | ≤48 |
| Embodiment two | 90.3 | 2.1 | 35 | ≤53 |
| Embodiment three | 93.7 | 1.4 | 20 | ≤32 |
| Example IV | 89.6 | 2.3 | 43 | ≤61 |
| Embodiment five | 91.5 | 1.7 | 26 | ≤31 |
| Embodiment six | 92.2 | 1.5 | 18 | ≤16 |
| Embodiment seven | 90.8 | 1.8 | 27 | ≤51 |
| Embodiment eight | 91.3 | 1.7 | 31 | ≤56 |
| Embodiment nine | 93.4 | 1.5 | 23 | ≤33 |
| Embodiment ten | 89.8 | 2.4 | 36 | ≤57 |
| Embodiment 11 | 90.5 | 2.2 | 33 | ≤43 |
| Embodiment 12 | 91.1 | 1.9 | 29 | ≤38 |
| Comparative example one | 87.5 | 3.5 | 57 | ≤71 |
| Comparative example two | 88.2 | 3.4 | 53 | ≤67 |
| Comparative example three | 85.4 | 4.1 | 67 | ≤74 |
| Comparative example four | 83.9 | 4.3 | 71 | ≤73 |
| Comparative example five | 86.5 | 3.9 | 61 | ≤65 |
| Comparative example six | 84.6 | 4.5 | 77 | ≤63 |
Can be seen that the capacitor prepared using the method for the present invention from the data of table 1 has high power capacity extraction rate, low damage
The small characteristic of consumption, low ESR (ESR), leakage current.
In comparative example, since water content is higher and includes glacial acetic acid (i.e. low pH value) in pretreatment fluid so that silane water
Solution acceleration, accelerates hydrolysis to trigger the polycondensation of silicone hydroxyl itself, and polymer chain increases the big particle diameter molecule of generation and is easy to block dielectric layer
Partial pore passage, be unfavorable for tantalum capacitor capacity draw, finally will also result in the hydraulic performance decline of capacitor；And in this hair
Due to including a large amount of solvents in bright so that silane is in dielectric layer surface fully penetrated, absorption, and since treatment fluid is low water content
Neutral liquid, a small amount of water and alcoholic extract hydroxyl group form hydrogen bond (wherein embodiment seven do not include into embodiment 12 in treatment fluid
Water, and by controlling high ambient humidity to provide hydrone for silane hydrolyzate) so that the hydrolysis rate of silane is eased, you can
So that silane coupling agent can by solvent siphonic effect by dielectric layer surface fully penetrated, absorption, in certain temperature
The organo-functional group to be formed and be included in silicone hydroxyl, and silane coupling agent is hydrolyzed under degree and promotes guide layer and conductive polymer layer
With stronger affinity；The hydrolysis rate of silane coupling agent is also controlled by reaction temperature at the same time, and dehydration is closed at high temperature
Into guide layer, the interface fusion of promotion guide layer and dielectric layer, so as to improve continuity, the densification that conducting polymer film layer is coated to
Property；In addition, by adding a small amount of aerosil in treatment fluid, it can cause aerosil and silane coupling agent
Good inorganic interface fusion is formed, can be with micropore invalid in filled media layer to prevent invalid micropore from influencing electricity
The Electrical Indexes of container.Therefore, the chip conducting polymer tantalum capacitor cathode guide manufactured by the manufacturing method of the present invention
Layer has high power capacity extraction rate, low-loss, low ESR and leakage come the chip polymer tantalum capacitor further prepared
The small characteristic of electric current.
Above content is that a further detailed description of the present invention in conjunction with specific preferred embodiments, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For those skilled in the art, do not taking off
On the premise of from present inventive concept, some equivalent substitutes or obvious modification can also be made, and performance or purposes are identical, all should
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, it is characterised in that comprise the following steps：
By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, with 0.01~5.0mm/min after 1~20min of dipping
Speed take out, place 5~30min at a temperature of 20~30 DEG C, and to form chip conductive for drying and forming-film at 50~260 DEG C
Polymer tantalum capacitor cathode guide layer；Wherein described treatment fluid include percentage by weight be 0.005~2.0% it is silane coupled
Agent, 0.01~0.1% aerosil, the solvent of 3~15% water and surplus.
2. manufacture method according to claim 1, it is characterised in that the solvent is included in alcohols, ketone, ethers extremely
Few one kind.
3. manufacture method according to claim 1, it is characterised in that the solvent includes methanol, ethanol, propyl alcohol, isopropyl
Alcohol, n-butanol, isobutanol, amylalcohol, lauryl alcohol, acetone, butanone, isophorone, methyl ether, ether, butyl ether, ethylene glycol monobutyl ether,
At least one of methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole.
4. manufacture method according to claim 1, it is characterised in that the general formula of the silane coupling agent is RnSiX4-n, its
Middle R is octenyl, dodecyl, urea groups, carbon alkoxy, cation alkyl, vinyl, amino, epoxy group, sulfydryl or acryloyl
Oxygen propyl group, X is alkoxy, aryloxy group, acyl group, methoxy or ethoxy.
5. manufacture method according to claim 1, it is characterised in that the silane coupling agent is amino silane, sulfydryl silicon
At least one of alkane, epoxy radicals silicone hydride, vinyl silanes, acryloxypropyl silane, dodecyl silane.
6. manufacture method according to any one of claims 1 to 5, it is characterised in that the treatment fluid includes weight percent
It is more molten than the silane coupling agent for 0.1~1.5%, 0.01~0.05% aerosil, 4~10% water and surplus
Agent.
7. manufacture method according to any one of claims 1 to 5, it is characterised in that the treatment fluid includes weight percent
Than the solvent of the silane coupling agent for 0.3~1.0%, 0.01~0.05% aerosil, 5~8% water and surplus.
8. manufacture method according to any one of claims 1 to 5, it is characterised in that by surface attachment Ta2O5Dielectric layer
Anode tantalum block is impregnated in treatment fluid after taking-up, and 20min is placed at a temperature of 20~25 DEG C, and dry at 170~210 DEG C
Film forming forms chip conducting polymer tantalum capacitor cathode guide layer.
9. a kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer, it is characterised in that comprise the following steps：
By surface attachment Ta2O5The anode tantalum block of dielectric layer is impregnated in treatment fluid, with 0.01~5.0mm/min after 1~20min of dipping
Speed take out, temperature at 20~30 DEG C, place 60~360min under the humidity of 50%RH~100%RH, and 50~260
Drying and forming-film forms chip conducting polymer tantalum capacitor cathode guide layer at DEG C；Wherein described treatment fluid includes percentage by weight
The solvent of silane coupling agent, 0.01~0.1% aerosil and surplus for 0.005~2.0%.
10. manufacture method according to claim 9, it is characterised in that the solvent includes methanol, ethanol, propyl alcohol, isopropyl
Alcohol, n-butanol, isobutanol, amylalcohol, lauryl alcohol, acetone, butanone, isophorone, methyl ether, ether, butyl ether, ethylene glycol monobutyl ether,
At least one of methyl tertiary butyl ether, ethyl methyl ether, methyl phenyl ethers anisole.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1341196A2 (en) * | 2002-02-27 | 2003-09-03 | Fuji Photo Film Co., Ltd. | Electrolytic composition, photoelectric conversion device and photoelectric cell |
| CN103390500A (en) * | 2013-07-30 | 2013-11-13 | 中国振华（集团）新云电子元器件有限责任公司 | Manufacturing method for solid electrolytic condenser with high puncture voltage |
| CN103500659A (en) * | 2013-10-16 | 2014-01-08 | 中国振华（集团）新云电子元器件有限责任公司 | Macromolecular polymerization tantalum capacitor cathode preparation method |
| CN103680961A (en) * | 2012-08-31 | 2014-03-26 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing tantalum capacitor |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1341196A2 (en) * | 2002-02-27 | 2003-09-03 | Fuji Photo Film Co., Ltd. | Electrolytic composition, photoelectric conversion device and photoelectric cell |
| CN103680961A (en) * | 2012-08-31 | 2014-03-26 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing tantalum capacitor |
| CN103390500A (en) * | 2013-07-30 | 2013-11-13 | 中国振华（集团）新云电子元器件有限责任公司 | Manufacturing method for solid electrolytic condenser with high puncture voltage |
| CN103500659A (en) * | 2013-10-16 | 2014-01-08 | 中国振华（集团）新云电子元器件有限责任公司 | Macromolecular polymerization tantalum capacitor cathode preparation method |
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